Solvent extraction process



Jan. -14, .19415 B. c. B ELDEN- 2,228,434

' SOLVENT EXTRACTION PROCESS med Junej4, 1938 2 sheets-sheet 1 ou. conf/Navas #HA-Sz vrfzow rusa E VL M CMSW Jan. 14,1941; m. BELDN 2,228,434

SOLVENT EXTRACTION PROCESS Filed June 4, 19:58 l2 sheets-sheet 2 f mm .I' '1| f '2 fj? '50 30; 28

.SPRAY Patented Jan. 14,1941

UNITED s'rii'n-:sf `P.'af'liailSn OFFICE sonvsar nx'riuic'rxonraociissv Burton G. Belden, Cranford, N. J., assigner to ration ot Delaware Standard Oil' Development Company, a corpo- Application .rune 4, 193s, serial No. 211,747

, v c "s claims. (Cl. 19e-13) The present invention relates to an improvedv y process of operating a solvent extraction tower or similar apparatus. It particularly relates, to a method of loperating extraction towers in which 5 at least one phase and preferably two phases are liquid. The improved process of the present invention is secured bycreating a surging or pulsating motion within Asaid'cxtraction tower .or similar apparatus.

It is well known in the art to operate towers or similar equipment in which a liquid and gas lor a. liquid. and liquid are commingled and are in intimate contact with each other and in which certain constituents 'of one phase are dissolved and removed in the other phase or phases. These processes as a general rule are carried out in towers which may contain catalytic or contact masses, packing members, dispersing trays, settling trays and the like. These processes are usually '20 conducted with countercurrent tlow in which one phase is introduced at the top oi'. the tower kand the other' at the bottom or in processes in which,

for instance, a third phase may be introduced'at another point on the tower. For example, a well known process of the type and especially petroleum lubricating oils. In this process the relatively more aromatic materials are separated from the relatively more paramnic iective solvents in orderv to secure a high quality lubricating oil. The usual method employed is to use solvents of the class which vhave a preferential selectivityfor the aromatic type'compounds and to intimately contact the appropriate solvent or solvent mixture under suitable conditions with the lubricating oil being treated. Solvents of this class are, for example, sulfur dioxide, fur-.- fural, aniline, phenol,.beta beta dichlorl diethyl 4Q ether, nitro benzene and the like. These ma'ybe employed in any desired combination or may be modified with regard to selectivity and solvent power bythe addition of inert solvents, as for example, by the addition of water, alcohols, or glydescribed, is a method of refining mineral oils' constituents of the lubricating oil by means of se' downwardly through' the .tower intimately contacting a vcountercurrently flowing oil phase which is fed into thebottom of the tower; rIn processes of this character, many devices have been tried in an attempt to secure more i'n imate and eiil.- 5 cient. contact between the respec ive phases and to secure a more rapid and cleaner separation for the purpose of improving the quality and yield,

' and Vfor the purpose ofincreasing the capacity of the particular .treating apparatus. For example, 10

to form at particular spots in the tower, as for instance, beneath plates and at other restricted points. These areas are characterized by partial 2Q or complete segregation of one of" the liquid phases and are therefore of limited usefulness for. phase-contacting purposes. Furthermore, if

'a catalyst or contact mass or pierced platesv and' the like areused, any carbonaceous or highly 25 viscous materials suspended in either liquid phase tend to settle on the surfaces and in the restricted passageways of the same, thereby descreasing the catalytic activity or tending to impair liquid flow l through the tower. 0 The process of the present invention not only overcomes these difficulties and disadvantages, .but also secures velocity pulses which improve the f dispersion of one phase in the other and also secure better distribution and mixing of the respective phases with consequent more'eifective carrying out of the extraction operation. The process of the present invention creates an intermittent pulsing motion within the tower by any 40 desirable means, as for example, by intermittent or irregular injection o i a particular phase or by' intermittent or irregular withdrawal of a particular fraction or fractions. The process of the present invention may be more readily understood by reference to the attached figures whichA are given for the purpose oi' illustrating several methods of conducting theprocess and which are not to be construed' as limiting the invention'inA any manner whatsoever. f v i and the discontinuous phases to pass around the distributing` plates. The raffinate layer is collected in section 9 land withdrawn through takeo line it, whereas the solvent extract layer is collected in section Il and withdrawn through line I4, being released through valve i5. j

In towers of this construction or of similar construction, local areas or zones of a particular phase collect and do not mix in a satisfactory manner with the otherA phase. For example, local, areas of the oil collect in zone I1 beneath the distributing plates 5. Furthermore, in towers of this construction in which a catalytic or contacting mass or other distributing means are employed, it has been observed that when treating certain grades of feed materials, a carbonaceous material settles on the contact or catalytic masses or distributingf'plates and tends to clog up the contact masses or to reduce the activity of the catalytic substances.

The process of the present invention overcomes this by causing a pulsing or vibratory motion of the entire liquid content of said tower. This may be accomplished by several methods or by a combination of various methods. For example, the feed may be introduced at a constant rate through line 4 and the solvent may be introduced at a constant rate through line 2, but control valve I5 may be adjusted to fully' open for an interval, thereby causing the entire liquid volume to move downwardly through the tower. This would cause a rapid movement throughout the tower and would disperse the zones below the distributing plates, since the downiiowing liquid would flow at a high velocity downwardly through both the downflow and upnow tubes By fully opening valve I5 it would cause a sufficient ve-4 locity and agitation in and around contact or catalytic masses which 'would tend to wash carbonaceous deposits off the same. Valve I5 at the end -of a certain interval could then be fully or partially closed. The preferred operation in regard to valve I5 would be to have the valve fully open for a period and then to fully 'ose the valve for a period three to four tim in length the time the valve was opened. These conditions, of course, can vary widely and will dependupon the respective feed rates, the'type of feed materials, the size, the volume and height ofthe tower, as well yas uponthe respective drawoff line sizes.

Another modification of the present invention' 4I5 may be hand operated or may be electrically operatedIv from a time clock or may beoperated by a device which fully opens when the interface level rises to a certain point in the` tower and closes when the interface level drops to a second lower point in the tower.

Another modication of the invention may be readily understood by reference to Figure 2. For purposes of simplicity, it is assumed that the material being treated is a petroleum oil of a lighter specific gravity than the solvent being used. In thisfigure, the selective solvent is introduced into tower 20 through feed line 2l and flows downwardly through the tower'intimately contacting the feed material flowing upwardly through the tower which is fed into tower 20 by means of feed line 22. The raffinate collects in section 23 of .the tower and is withdrawn through take-off line 24. The solvent extract collects in section 25 andis withdrawn through line 2S controlledby means of valve 21. In this tower' the downilowing solvent is distributed over plates 28'and flows through spouts 25. The upfiowing oil is collected under plates 28 and ows upwardly and is dispersed by means of the oil phase sprays 30. The operation of a tower of this or similar construction in accordance with the present invention is to withdraw the solvent extract phase at a relatively uniform rate throughline 28 controlled by valve 21 which may be hand operated or controlled in any other manner desirable, as for example, by electrical contacts which maintain the interface level at a utilized, as for example, centrifugal pumps or pressure equipment. Tower 20 may contain contact or catalytic masses or any.other means for distributing or directing the respective phases.

By operating the tower in the manner described, it is possible to greatly increase the velocity through the oil phase sprays, thereby getting considerably greater dispersion and also causing agitation throughout the tower which greatly increases the emciency and the capacity of the equipment.

The following example is given for purposes of illustrating the invention and is not to be con? strued as limiting the invention in any manner whatsoever.

Example In a solvent treating operation conducted in a tower containing suitable distributing and contacting means, a lubricating oil fraction is fed into the bottom of the tower. The oil ows up- Vwardly through .the tower intimatelycontacting vdownilowing phenol which is introduced into the top of the tower. 'I'he phenol is the continuous phase and the interface `between the solvent :rich layer and the solvent poor layer is maintained in the section above the solvent feed inlet. 'Ihe interface is permitted to rise from an initial point above the solvent feed inlet of the tower .at a gradual relatively slow rate to a second pre-determined point above the startingl point. When the interface level reaches the second pre-determined point, suitable means are employed to open a valve in the solvent extract take-oi! line. thereby causing the interface level to fall rapidvly to the lower initial starting point, at which 75 level suitable means are provided to activate the release valve on the solvent extract take-off line, restricting the flow and thus causingu the interface to rise and pass through similar succeeding cycles. y

The following data serve to illustrate the above method of operating:

Table Unit vols. Unit vols. Unit vols. Unit vois. -Unit time oi lube oil oi benol of raiiinate oi extract feed eed removed removed l 2 1 0 1 2 l 0 1 2 l 6 l 2 l 0 l 2 l 0 1 2 1 6 The above example illustrates a process in which the solventl extract release valve is fully closed for several unit times and then opened sufficiently for an initial unit time to remove the solvent extract accumulated for both periods.v A The operation may be varied so that the solvent extract valve may be partially open at all times and at periodic intervals fully open to create a surging or pulsating motion. It is to. be noted that in the abovelexample the raffinate is removed at a uniform' rate. This is accomplished by pumping or may also be accomplished byI having a raffinate reservoir in the tower above the point at which the ramnate is withdrawn so that when the liquid level inV the tower falls there will as. for'instance, from a .point immediately above' the oil inlet to a point from three inches to twenty-four inches over the initial point during the period from one minute to ten minutes and then to allow the interface level to drop from the upper point to the starting point duringa period from one-quarterto one-half the time'it took to build up. .y

It was found that when the tower was operated in accordance with the present invention. the catalytic and contact masses remained clear'and contained no adhered or -deposited 'matten When operated under a normal method in which a relatively vuniform flow was maintained. these contact masses.- pierced plates and catalytic masses accumulateddeposited and adhered mat.

ter which necessitated occasional shutdowns of the apparatus invorder to clean the same. It was furthermore found that when an operation was conducted in a' manner of the present invention,

` 3 more intimate contactV between the respective phases was secured which resulted in a better and cleaner separation and which increased the capacity of the apparatus.

The invention is not to be limited by any theory or mode of operation, but only by the following l claims. in which it is desired to claim all novelty insofar as the prior art permits.

I claim:

l. Improved process of operating a countercurrent solvent treating tower in which phenol is introduced into the top of the tower and oil is introduced into the bottom of the tower, comprising allowing the interface betweenl the respective layers to rise slowly from an initial point to a pre-determined point above the initial point and then allowing the interface to fall rapidly to the initial point by means of intermittently withdrawing one phase.

2. Process of operating ,a ccuntercurrent solvent treating tower in which a petroleum oil is contacted with a solvent under conditions to form a rafllnate ,phase and a solvent extract iace level in an initial stage rises from about 3 `to 24 inches during, altime period of from 1 to 10 minutes and in a secondary stage falls the distance through which it rose in about one-half the time required to rise. i

3.`Process of operating a countercurrent solvent treating tower in which a petroleum oil is contacted with a solvent under conditions to form a raflinate phase and a solvent extract phase, comprising adjusting the feed and withdrawal rates of said tower so that the interface level in an initial stage rises slowly over a flx'ed distance and in a secondary stage drops rapidly over said xed distance. v l

4. Process in accordance with claim 3 in which the time required for said interface level to fall `over vsaid ixed distance is less than one-half of.

the time required for said interface level to rise over said fixed distance. l

5. Process of operating a countercurrentvsolvent treating tower in which a petroleum oil is contacted with a solvent under conditions to form a rainate phase and a solvent extract phase, comprising adjusting the feed and withdrawal `rates of said tower so that theinterface level in an initial stage changes slowlyvin a positive direction over a fixed distance and in a secondary stage changes rapidly in a negative direction over said fixed distance.

6. Process in accordance with claim 5 in which rection over said iixed distance.

Un'roN c. BnmEN.' r 

